A kind of anti-flaming thermal-insulation multilayer film
Technical field
The present invention relates to fire proofing technical field, particularly relate to a kind of anti-flaming thermal-insulation multilayer film.
Background technology
At present, the building film that world architecture industry uses every year about has several hundred million square metres, and due to its low production cost, during construction, attachment is convenient, be more convenient for changing, and decoration kind is rich and varied, does not have light pollution, is had an optimistic view of by increasing foreign real estate business and owner.The country such as the U.S., Germany adopts state-of-the-art sputter coating technology in the world, there is very large market in the world, this is a kind of product collecting vacuum technique, plasma technology, gas discharge technology and the technology such as thin film physics, fine chemistry industry, but corresponding sputter coating technology also costly.
The development of building glass window explosion-proof insulated film originates from the seventies.The Experiment of Thermophysics display of a building, 1/3 of whole building heat loss is scattered and disappeared by windowpane, and glass explosion-proof insulated film is energy-conservation very effective.The preparation of inflaming retarding membrane mainly comprises following methods: a kind of is that the fire-retardant adhering resin containing a large amount of fire retardant is scattered in the surface after in solvent, it being coated on base material film, obtained composite membrane after solvent flashing.But need to add a large amount of fire retardants inside goods in the process of preparation, thus just can reach fire-retardant object, the interpolation of a large amount of fire retardant can have an impact to aspects such as the mechanical performances of goods; The fire retardant simultaneously used has the product of halogen often, can produce endotoxin contamination environment when burning.Second method is that the surface fire-retardant film being directly pressed on base material film obtains composite membrane.The inflaming retarding membrane that the method adopts is generally polyvinyl chloride, and this material can produce strong carcinogenic bioxin in the process of burning, and thus cannot meet the requirement of product environmental protection.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of anti-flaming thermal-insulation multilayer film, avoids using polyvinyl chloride, and good flame retardation effect, light transmittance is high.
In view of this; the invention provides a kind of anti-flaming thermal-insulation multilayer film; comprise the PETG diaphragm, acrylate glue adhensive layer, polyimide layer, heat insulating coat, organic silicon coating, organic silica gel adhensive layer and the explosion-proof rete that set gradually; described heat insulating coat is formed by insulating moulding coating, and described insulating moulding coating is prepared as follows:
Nano aluminium oxide, nano ceric oxide, gallium-doped zinc oxide and cerium acid yttrium system inorganic pigment is added in the first mixed solution, after dispersion treatment, surface modification and ball-milling treatment, obtain heat insulation nano composite mortar successively, described first mixed solution comprises ethanol, n-octyl alcohol, natrium citricum, polyethylene glycol and deionized water;
By described heat insulation nano composite mortar, polyurethane resin, levelling agent and and defoamer mixing, obtain insulating moulding coating after dispersion.
Preferably, the weight ratio of described nano aluminium oxide, nano ceric oxide, gallium-doped zinc oxide, cerium acid yttrium system inorganic pigment and polyurethane resin is 5-10:5-8:5-8:2-4:400-500.
Preferably, obtain in the step of heat insulation nano composite mortar, described dispersion treatment is specially: with the Rate Dispersion 5-10 minute of 300-500rpm.
Preferably, described gallium-doped zinc oxide is prepared as follows:
Solution of zinc sulfate and gallium nitrate solution are placed in reaction vessel, stir, adjust the temperature to 50 DEG C, then add polyethylene glycol, drip ammonia spirit, ultrasonic disperse 10-20 minute, continue reaction 20 minutes, stop stirring, leave standstill aging 1 hour under normal temperature, obtain white product;
By described white product centrifugation, wash 3 times respectively with deionized water and ethanolic solution, dry, 200-400 DEG C of calcining 2 hours, after grinding, obtain gallium-doped zinc oxide.
Preferably, described cerium acid yttrium system inorganic pigment is prepared as follows:
The yttrium nitrate of the cerous nitrate of 10-15 weight portion, 3-5 weight portion, the ferric sulfate of 0.5 weight portion are added in the deionized water of 100 weight portions, 5min is stirred under 300rpm, add the lemon acid amide of 2 weight portions, continue to stir 10min, then add the polyacrylamide of 3-5 weight portion and the glucose of 0.2-0.5 weight portion, obtain the second mixed solution;
By described second mixed solution stirring reaction 2 hours at water-bath 75-85 DEG C, obtain gel;
The constant temperature oven that described gel is placed in 120 DEG C is dried, calcines 4 hours at 200 DEG C, after grinding, obtain cerium acid yttrium system inorganic pigment.
Preferably, described organic silicon coating is formed by organosilicon coating, and described organosilicon coating is prepared as follows:
By the nano silicon of 5-6 weight portion, the nano titanium oxide of 6-7 weight portion is added in the mixed solution of ethanol and deionized water, add the glacial acetic acid of 0.2 weight portion, drip 4 parts by weight epoxy silane couplers, then the polysorbas20 of 0.3 weight portion is added, the isopropyl alcohol of 1 weight portion, the defoamer of 1 weight portion, with the speed stirring at normal temperature 20-30min of 300-500rpm, then the organic siliconresin of 20-30 weight portion is added, to obtain organosilicon coating after the speed stirring at normal temperature 20-30min of 300-500rpm.
Preferably, described explosion-proof rete adopts following raw material to prepare:
60-80 weight portion polyvinyl chloride, 5-8 weight portion dimethyl terephthalate (DMT), 10-20 weight portion PTT, 4-6 parts by weight of polyurethane elastomer, 4-8 parts by weight of dimethyldimethoxysil,ne, 6-8 parts by weight of plasticizer, 5-10 parts by weight of phosphoric acid triphenylmethyl methacrylate, 2-3 weight portion carboxyethyl phenyl phosphoric acid, 4-7 weight portion algaroth, nano-filled dose of 2-4 weight portion, 0.4-0.8 weight portion antioxidant 1010,1-2 weight portion polycarboimide stabilizing agent.
Preferably, described explosion-proof rete is prepared as follows:
60-80 weight portion polyvinyl chloride, 5-8 weight portion dimethyl terephthalate (DMT), 10-20 weight portion PTT, 4-6 parts by weight of polyurethane elastomer, 4-8 parts by weight of dimethyldimethoxysil,ne and 6-8 parts by weight of plasticizer are mixed, stir 10-20min with the rotating speed of 800-1000 rev/min, obtain the first mixture;
Described first mixture is heated to 80-90 DEG C, add 5-10 parts by weight of phosphoric acid triphenylmethyl methacrylate, 2-3 weight portion carboxyethyl phenyl phosphoric acid, 4-7 weight portion algaroth, nano-filled dose of 2-4 weight portion, 0.4-0.8 weight portion antioxidant 1010,1-2 weight portion polycarboimide stabilizing agent, after stirring 20-30min, obtain the second mixture;
Added in double screw extruder by described second mixture and carry out melt blending, extrude, cool, obtain pad pasting master batch after granulation, head temperature is 210 ~ 230 DEG C, screw speed 200 ~ 220r/min; Extrude through double screw extruder, after biaxial tension, obtain explosion-proof rete.
Preferably, described algaroth is prepared as follows:
At 40-45 DEG C, by 20 weight portion trichloride antimonies and the mixing of 30 weight portion red fuming nitric acid (RFNA)s, slowly add 45 weight portion antimony oxides, be heated to 100-115 DEG C, return stirring 1-1.5 hour, cooling, filters, and washing, obtains algaroth after drying.
Preferably, described nano-filled dose is nano-calcium carbonate.
The invention provides a kind of anti-flaming thermal-insulation multilayer film; comprise the PETG diaphragm, acrylate glue adhensive layer, polyimide layer, heat insulating coat, organic silicon coating, organic silica gel adhensive layer and the explosion-proof rete that set gradually; described heat insulating coat is formed by insulating moulding coating, described insulating moulding coating with nano aluminium oxide, nano ceric oxide, gallium-doped zinc oxide, cerium acid yttrium system inorganic pigment, polyurethane resin, levelling agent and and defoamer be prepared for raw material.Compared with prior art, the gallium-doped zinc oxide that the present invention adopts has the excellent optical performance of high reflectance in infrared light district.Secondly, cerium acid yttrium system inorganic pigment is not containing any heavy metal element, and environmental sound, has good resistance to elevated temperatures and physical and chemical stability, has very high reflectivity and chromatic value.Again, the explosion-proof rete that the present invention adopts has good fire resistance.Experimental result shows, the present invention avoids using polyvinyl chloride, and the anti-flaming thermal-insulation multilayer film provided, good flame retardation effect, light transmittance is high.
Detailed description of the invention
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of anti-flaming thermal-insulation multilayer film, comprise the PETG diaphragm set gradually, acrylate glue adhensive layer, polyimide layer, heat insulating coat, organic silicon coating, organic silica gel adhensive layer and explosion-proof rete, described heat insulating coat is formed by insulating moulding coating, described insulating moulding coating is prepared as follows: by nano aluminium oxide, nano ceric oxide, gallium-doped zinc oxide and cerium acid yttrium system inorganic pigment are added in the first mixed solution, successively through dispersion treatment, heat insulation nano composite mortar is obtained after surface modification and ball-milling treatment, described first mixed solution comprises ethanol, n-octyl alcohol, natrium citricum, polyethylene glycol and deionized water, by described heat insulation nano composite mortar, polyurethane resin, levelling agent and and defoamer mixing, obtain insulating moulding coating after dispersion.
In the preparation process of insulating moulding coating, the weight ratio of described nano aluminium oxide, nano ceric oxide, gallium-doped zinc oxide, cerium acid yttrium system inorganic pigment and polyurethane resin is preferably 5-10:5-8:5-8:2-4:400-500, is more preferably 6-9:6-8:5-7:3-4:420-480.
Obtain in the step of heat insulation nano composite mortar, described dispersion treatment is specially: with the Rate Dispersion 5-10 minute of 300-500rpm; Described ball-milling treatment is specially: utilize ball mill grinding 20-30 minute.Described surface modification step is specially: dropwise drip silane coupler, and wherein, the silane coupler that the present invention adopts is preferably silane coupler KH570.
In described first mixed solution, the weight ratio of ethanol, n-octyl alcohol, natrium citricum, polyethylene glycol and deionized water is preferably 30-50:6-15:3-7:3-7:40-60, is more preferably 40:10:5:4:50.
Preferably, described gallium-doped zinc oxide is prepared as follows: solution of zinc sulfate and gallium nitrate solution are placed in reaction vessel, stir, adjust the temperature to 50 DEG C, then add polyethylene glycol, drip ammonia spirit, ultrasonic disperse 10-20 minute, continues reaction 20 minutes, stops stirring, leave standstill aging 1 hour under normal temperature, obtain white product; By described white product centrifugation, and wash 3 times respectively with deionized water and ethanolic solution, dry, 200-400 DEG C of calcining 2 hours, after grinding, obtain gallium-doped zinc oxide.
Preferably, described cerium acid yttrium system inorganic pigment is prepared as follows: be added in the deionized water of 100 weight portions by the yttrium nitrate of the cerous nitrate of 10-15 weight portion, 3-5 weight portion, the ferric sulfate of 0.5 weight portion, 5min is stirred under 300rpm, add the lemon acid amide of 2 weight portions, continue to stir 10min, then add the polyacrylamide of 3-5 weight portion and the glucose of 0.2-0.5 weight portion, obtain the second mixed solution; By described second mixed solution stirring reaction 2 hours at water-bath 75-85 DEG C, obtain gel; The constant temperature oven that described gel is placed in 120 DEG C is dried, calcines 4 hours at 200 DEG C, after grinding, obtain cerium acid yttrium system inorganic pigment.
According to the present invention, gallium-doped zinc oxide has the excellent optical performance of high reflectance in infrared light district.Cerium acid yttrium system inorganic pigment is preferably white, it is not containing any heavy metal element, environmental sound, rare earth material can change himself color characteristics by charge transfer transition mode between transition metal, take on the role of donor level and acceptor level at charge transtion rare earth elements and transition metal respectively.After doping chromogenic agent element, sample visible region absorbs limit to be increased gradually, and then causes the increase along with element doping amount, and energy gap Eg also reduces gradually.The present invention is using rare-earth yttrium oxide as additive, and using ceria as host material, prepare fire-resistant nontoxic pigment, this pigment has good resistance to elevated temperatures and physical and chemical stability, has very high reflectivity and chromatic value.
Preferably, described organic silicon coating is formed by organosilicon coating, described organosilicon coating is prepared as follows: by the nano silicon of 5-6 weight portion, the nano titanium oxide of 6-7 weight portion is added in the mixed solution of ethanol and deionized water, add the glacial acetic acid of 0.2 weight portion, drip 4 parts by weight epoxy silane couplers, then the polysorbas20 of 0.3 weight portion is added, the isopropyl alcohol of 1 weight portion, the defoamer of 1 weight portion, with the speed stirring at normal temperature 20-30min of 300-500rpm, then the organic siliconresin of 20-30 weight portion is added, to obtain organosilicon coating after the speed stirring at normal temperature 20-30min of 300-500rpm.
Preferably, described explosion-proof rete adopts following raw material to prepare: 60-80 weight portion polyvinyl chloride, 5-8 weight portion dimethyl terephthalate (DMT), 10-20 weight portion PTT, 4-6 parts by weight of polyurethane elastomer, 4-8 parts by weight of dimethyldimethoxysil,ne, 6-8 parts by weight of plasticizer, 5-10 parts by weight of phosphoric acid triphenylmethyl methacrylate, 2-3 weight portion carboxyethyl phenyl phosphoric acid, 4-7 weight portion algaroth, nano-filled dose of 2-4 weight portion, 0.4-0.8 weight portion antioxidant 1010,1-2 weight portion polycarboimide stabilizing agent.
Preferably, described explosion-proof rete is prepared as follows: 60-80 weight portion polyvinyl chloride, 5-8 weight portion dimethyl terephthalate (DMT), 10-20 weight portion PTT, 4-6 parts by weight of polyurethane elastomer, 4-8 parts by weight of dimethyldimethoxysil,ne and 6-8 parts by weight of plasticizer are mixed, stir 10-20min with the rotating speed of 800-1000 rev/min, obtain the first mixture; Described first mixture is heated to 80-90 DEG C, add 5-10 parts by weight of phosphoric acid triphenylmethyl methacrylate, 2-3 weight portion carboxyethyl phenyl phosphoric acid, 4-7 weight portion algaroth, nano-filled dose of 2-4 weight portion, 0.4-0.8 weight portion antioxidant 1010,1-2 weight portion polycarboimide stabilizing agent, after stirring 20-30min, obtain the second mixture; Added in double screw extruder by described second mixture and carry out melt blending, extrude, cool, obtain pad pasting master batch after granulation, head temperature is 210 ~ 230 DEG C, screw speed 200 ~ 220r/min; Extrude through double screw extruder, after biaxial tension, obtain explosion-proof rete.
Described algaroth is preferably prepared as follows: at 40-45 DEG C, by 20 weight portion trichloride antimonies and the mixing of 30 weight portion red fuming nitric acid (RFNA)s, slowly add 45 weight portion antimony oxides, be heated to 100-115 DEG C, return stirring 1-1.5 hour, cooling, filtered, washing, obtains algaroth after drying.Preferably, described nano-filled dose is nano-calcium carbonate.
A lot of performances of described PTT (being called for short PTT) are between PET and PBT, ptt fiber combines flexibility, the bulkiness of acrylic fibers, the pollution resistance of terylene of nylon, add elasticity inherently, and can the feature such as normal temperature dyeing, the premium properties of various fiber is rolled into one.Adding of dimethyldimethoxysil,ne makes polyvinyl chloride, polyurethane elastomer and dimethyl terephthalate (DMT) can have good graft reaction and compatibility with other material.
Adding of described dimethyldimethoxysil,ne makes whole system have better percent grafting, polyvinyl chloride, PTT and polyurethane elastomer is made to have good compatibility, impel polyvinyl chloride, PTT and polyurethane elastomer to form the structure of interpenetrating networks makes the mechanical performance of film get a promotion simultaneously, simultaneously the dispersiveness of each component in also raising system.
Described nano-filled dose can the paradigmatic structure of strengthening material, improve the performance such as bending modulus, robustness, tensile strength, ductility, shear strength, shock resistance, compression strength of product, also can reduce production cost.Described nano-filled dose is preferably nano-calcium carbonate.
The present invention is using algaroth as inorganic antimony fire retardant, itself has fire retardation, with halide-containing with the use of time, there is excellent flame retardant synergism equally, as compared to the inorganic antimony compounds such as conventional antimony oxide and sodium antimonate, there is more excellent flame-retarded efficiency and range of application more widely.Moreover, algaroth is less on the impact of the transparency of high polymer, and what this made antimony oxychlorides as flame retardants adds the light transmission that can not change film.
Above-mentioned anti-flaming thermal-insulation multilayer film is preferably adopted and is prepared with the following method:
PETG diaphragm is provided;
At described PETG diaphragm surface coating acrylic acid adhesive, form acrylate glue adhensive layer;
Polyimide film is fitted on described acrylate glue adhensive layer, form polyimide layer;
At described polyimide surface successively coating thermal insulating and organosilicon coating, form heat insulating coat and organic silicon coating respectively;
Stick agent at described organic silicon coating surface coating organic silica gel, form organic silica gel adhensive layer;
Rupture pressure disc is fitted in described organosilicon adhesive surface, form explosion-proof rete, obtain anti-flaming thermal-insulation multilayer film.
As can be seen from above scheme, the invention provides a kind of anti-flaming thermal-insulation multilayer film, the gallium-doped zinc oxide of employing has the excellent optical performance of high reflectance in infrared light district.Secondly, cerium acid yttrium system inorganic pigment is not containing any heavy metal element, and environmental sound, has good resistance to elevated temperatures and physical and chemical stability, has very high reflectivity and chromatic value.Again, the explosion-proof rete that the present invention adopts has good fire resistance.Experimental result shows, the present invention avoids using polyvinyl chloride, and the anti-flaming thermal-insulation multilayer film provided, good flame retardation effect, light transmittance is high.
In order to understand the present invention further, be described in detail to technical scheme provided by the invention below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
The raw material that the embodiment of the present invention adopts and chemical reagent are commercial.
Embodiment 1
The preparation process of gallium-doped zinc oxide is as follows:
Measure the solution of zinc sulfate (1moL/L) of 20 weight portions, the gallium nitrate solution (0.2moL/L) of 10 weight portions is placed in beaker, be placed in by flask on magnetic stirring apparatus and stir, adjust the temperature to 50 DEG C, the polyethylene glycol taking 2-4 weight portion adds in beaker, ammonia spirit is dripped to beaker, be precipitated, by white precipitate ultrasonic disperse 20 minutes, continue reaction 20 minutes, stop stirring, under normal temperature, leave standstill aging 1 hour.By the centrifugation of white precipitate product, and wash 3 times respectively with deionized water and ethanolic solution, sediment was in baking oven 6 hours, and finally 200 DEG C of calcinings two hours in Muffle furnace, namely grinding obtains gallium-doped zinc oxide powder.
The preparation method of cerium acid yttrium system inorganic pigment comprises the steps:
The yttrium nitrate of the cerous nitrate of 12 weight portions, 4 weight portions, the ferric sulfate of 0.5 weight portion are joined in the deionized water of 100 weight portions, 5min is stirred under 300rpm, add the lemon acid amide of 2 weight portions, continue to stir 10min, then add the polyacrylamide of 3 weight portions and the glucose of 0.5 weight portion.Then by mixed solution stirring reaction 2 hours at water-bath 85 DEG C.Dried by the constant temperature oven that above-mentioned gel is placed in 120 DEG C, obtain semi-finished product, calcine 4 hours at semi-finished product being placed in Muffle furnace 200 DEG C, grinding obtains cerium acid yttrium system inorganic pigment.
Insulating moulding coating is prepared as follows:
The ethanol of S1,40 weight portions, the n-octyl alcohol of 10 weight portions, the natrium citricum of 5 weight portions, the polyethylene glycol of 4 weight portions, in the deionized water of 50 weight portions, add the nano aluminium oxide of 6 weight portions, the nano ceric oxide of 6 weight portions, the gallium-doped zinc oxide of 6 weight portions, the cerium acid yttrium system inorganic pigment of 3 weight portions, 400rpm disperses 8 minutes, then dropwise drips the silane coupler (KH570) of 10 weight portions, then use ball mill grinding 20-30 minute, make heat insulation nano composite material powdery pulp.
S2, get the polyurethane resin of 450 weight portions, add above-mentioned heat-insulating slurry, add the coating high speed dispersor of heat-insulating slurry at 800 rpm, disperse 30 minutes, then add the levelling agent of 2 weight portions, the defoamer of 2 weight portions, continue dispersion 20 minutes, be prepared into insulating moulding coating.
The present embodiment provides a kind of preparation method of organosilicon coating, comprises the steps:
By the nano silicon of 5 weight portions, the nano titanium oxide of 6 weight portions joins in the deionized water of ethanol containing 20 weight portions and 30 weight portions, add the glacial acetic acid of 0.2 weight portion, drip 4 weight portion KH560 (epoxy silane coupling agent), then add the polysorbas20 of 0.3 weight portion, the isopropyl alcohol of 1 weight portion, the defoamer of 1 weight portion, stirring at normal temperature 30min under 400rpm, adds the organic siliconresin of 30 weight portions, stirring at normal temperature 30min under 400rpm, obtains organosilicon coating.
The present embodiment provides a kind of preparation method of rupture pressure disc, comprises the steps:
L1, algaroth preparation method: at 42 DEG C, by 20 weight portion trichloride antimonies and the mixing of 30 weight portion red fuming nitric acid (RFNA)s, slowly add 45 weight portion antimony oxides, be heated to 105 DEG C, return stirring 1 hour, cooling, filter, washing, obtains algaroth after drying.
L2, the present invention also provide a kind of preparation method of rupture pressure disc, with parts by weight, comprise the following steps: by 78 weight portion polyvinyl chloride, 6 weight portion dimethyl terephthalate (DMT)s, 13 weight portion PTTs, 5 parts by weight of polyurethane elastomers, 6 parts by weight of dimethyldimethoxysil,ne, 7 parts by weight of plasticizer mixing, stir 20min with the rotating speed of 900 revs/min, obtain the first mixture; Described first mixture is heated to 90 DEG C, add 6 parts by weight of phosphoric acid triphenylmethyl methacrylates, 3 weight portion carboxyethyl phenyl phosphoric acid, 6 weight portion algaroths, nano-filled dose of 3 weight portions, 0.6 weight portion antioxidant (1010), 1 weight portion polycarboimide stabilizing agent, after stirring 30min, obtain the second mixture; Added in double screw extruder by described second mixture and carry out melt blending, extrude, cool, obtain pad pasting master batch after granulation, head temperature is 210 ~ 230 DEG C, screw speed 200 ~ 220r/min; Extrude through double screw extruder, after biaxial tension, obtain rupture pressure disc.
The preparation process of anti-flaming thermal-insulation multilayer film is as follows:
PETG diaphragm is provided;
At described PETG diaphragm surface coating acrylic acid adhesive, form acrylate glue adhensive layer;
Polyimide film is fitted on described acrylate glue adhensive layer, form polyimide layer;
At described polyimide surface successively coating thermal insulating and organosilicon coating, form heat insulating coat and organic silicon coating respectively;
Stick agent at described organic silicon coating surface coating organic silica gel, form organic silica gel adhensive layer;
Rupture pressure disc is fitted in described organosilicon adhesive surface; form explosion-proof rete; obtain anti-flaming thermal-insulation multilayer film, described anti-flaming thermal-insulation multilayer film comprises the explosion-proof rete of 1.PET diaphragm 2. acrylate glue adhensive layer 3. polyimide layer 4. heat insulating coat 5. organic silicon coating 6. organic silica gel adhensive layer 7. set gradually.
Embodiment 2
The preparation process of gallium-doped zinc oxide is as follows:
Measure the solution of zinc sulfate (1moL/L) of 20 weight portions, the gallium nitrate solution (0.2moL/L) of 10 weight portions is placed in beaker, be placed in by flask on magnetic stirring apparatus and stir, adjust the temperature to 50 DEG C, the polyethylene glycol taking 3 weight portions adds in beaker, ammonia spirit is dripped to beaker, be precipitated, by white precipitate ultrasonic disperse 12 minutes, continue reaction 20 minutes, stop stirring, under normal temperature, leave standstill aging 1 hour.By the centrifugation of white precipitate product, and wash 3 times respectively with deionized water and ethanolic solution, sediment was in baking oven 6 hours, and finally 300 DEG C of calcinings two hours in Muffle furnace, namely grinding obtains gallium-doped zinc oxide powder.
The preparation method of cerium acid yttrium system inorganic pigment comprises the steps:
The yttrium nitrate of the cerous nitrate of 10-15 weight portion, 3-5 weight portion, the ferric sulfate of 0.5 weight portion are joined in the deionized water of 100 weight portions, 5min is stirred under 300rpm, add the lemon acid amide of 2 weight portions, continue to stir 10min, then add the polyacrylamide of 4 weight portions and the glucose of 0.3 weight portion.Then by mixed solution stirring reaction 2 hours at water-bath 75 DEG C.Dried by the constant temperature oven that above-mentioned gel is placed in 120 DEG C, obtain semi-finished product, calcine 4 hours at semi-finished product being placed in Muffle furnace 200 DEG C, grinding obtains cerium acid yttrium system inorganic pigment.
Insulating moulding coating is prepared as follows:
The ethanol of S1,40 weight portions, the n-octyl alcohol of 10 weight portions, the natrium citricum of 5 weight portions, the polyethylene glycol of 4 weight portions, in the deionized water of 50 weight portions, add the nano aluminium oxide of 6 weight portions, the nano ceric oxide of 5 weight portions, the gallium-doped zinc oxide of 8 weight portions, the cerium acid yttrium system inorganic pigment of 3 weight portions, 300rpm disperses 5 minutes, then dropwise drips the silane coupler (KH570) of 6 weight portions, then use ball mill grinding 20-30 minute, make heat insulation nano composite material powdery pulp.
S2, get the polyurethane resin of 400 weight portions, add above-mentioned heat-insulating slurry, add the coating high speed dispersor of heat-insulating slurry at 800 rpm, disperse 20 minutes, then add the levelling agent of 2 weight portions, the defoamer of 1 weight portion, continue dispersion 16 minutes, be prepared into insulating moulding coating.
The present embodiment provides a kind of preparation method of organosilicon coating, comprises the steps:
By the nano silicon of 5 weight portions, the nano titanium oxide of 6 weight portions joins in the deionized water of ethanol containing 20 weight portions and 30 weight portions, add the glacial acetic acid of 0.2 weight portion, drip 4 weight portion KH560 (epoxy silane coupling agent), then the polysorbas20 of 0.3 weight portion is added, the isopropyl alcohol of 1 weight portion, the defoamer of 1 weight portion, stirring at normal temperature 20-30min under 500rpm, add the organic siliconresin of 20-30 weight portion, stirring at normal temperature 20min under 500rpm, obtains organosilicon coating.
The present embodiment provides a kind of preparation method of rupture pressure disc, comprises the steps:
L1, algaroth preparation method: at 45 DEG C, by 20 weight portion trichloride antimonies and the mixing of 30 weight portion red fuming nitric acid (RFNA)s, slowly add 45 weight portion antimony oxides, be heated to 100 DEG C, return stirring 1.5 hours, cooling, filter, washing, obtains algaroth after drying.
L2, the present invention also provide a kind of preparation method of rupture pressure disc, with parts by weight, comprise the following steps: by 65 weight portion polyvinyl chloride, 7 weight portion dimethyl terephthalate (DMT)s, 12 weight portion PTTs, 4 parts by weight of polyurethane elastomers, 5 parts by weight of dimethyldimethoxysil,ne, 6 parts by weight of plasticizer mixing, stir 20min with the rotating speed of 1000 revs/min, obtain the first mixture; Described first mixture is heated to 90 DEG C, add 5 parts by weight of phosphoric acid triphenylmethyl methacrylates, 3 weight portion carboxyethyl phenyl phosphoric acid, 6 weight portion algaroths, nano-filled dose of 3 weight portions, 0.8 weight portion antioxidant (1010), 2 weight portion polycarboimide stabilizing agents, after stirring 30min, obtain the second mixture; Added in double screw extruder by described second mixture and carry out melt blending, extrude, cool, obtain pad pasting master batch after granulation, head temperature is 210 ~ 230 DEG C, screw speed 200 ~ 220r/min; Extrude through double screw extruder, after biaxial tension, obtain rupture pressure disc.
The preparation process of anti-flaming thermal-insulation multilayer film is as follows:
PETG diaphragm is provided;
At described PETG diaphragm surface coating acrylic acid adhesive, form acrylate glue adhensive layer;
Polyimide film is fitted on described acrylate glue adhensive layer, form polyimide layer;
At described polyimide surface successively coating thermal insulating and organosilicon coating, form heat insulating coat and organic silicon coating respectively;
Stick agent at described organic silicon coating surface coating organic silica gel, form organic silica gel adhensive layer;
Rupture pressure disc is fitted in described organosilicon adhesive surface; form explosion-proof rete; obtain anti-flaming thermal-insulation multilayer film, described anti-flaming thermal-insulation multilayer film comprises the explosion-proof rete of 1.PET diaphragm 2. acrylate glue adhensive layer 3. polyimide layer 4. heat insulating coat 5. organic silicon coating 6. organic silica gel adhensive layer 7. set gradually.
Embodiment 3
The preparation process of gallium-doped zinc oxide is as follows:
Measure the solution of zinc sulfate (1moL/L) of 20 weight portions, the gallium nitrate solution (0.2moL/L) of 10 weight portions is placed in beaker, be placed in by flask on magnetic stirring apparatus and stir, adjust the temperature to 50 DEG C, the polyethylene glycol taking 3 weight portions adds in beaker, ammonia spirit is dripped to beaker, be precipitated, by white precipitate ultrasonic disperse 10 minutes, continue reaction 20 minutes, stop stirring, under normal temperature, leave standstill aging 1 hour.By the centrifugation of white precipitate product, and wash 3 times respectively with deionized water and ethanolic solution, sediment was in baking oven 6 hours, and finally 200 DEG C of calcinings two hours in Muffle furnace, namely grinding obtains gallium-doped zinc oxide powder.
The preparation method of cerium acid yttrium system inorganic pigment comprises the steps:
The ferric sulfate of the cerous nitrate of 12 weight portions, the yttrium nitrate of 4 weight portions, 0.5 weight portion joins in the deionized water of 100 weight portions, 5min is stirred under 300rpm, add the lemon acid amide of 2 weight portions, continue to stir 10min, then add the polyacrylamide of 3 weight portions and the glucose of 0.5 weight portion.Then by mixed solution stirring reaction 2 hours at water-bath 85 DEG C.Dried by the constant temperature oven that above-mentioned gel is placed in 120 DEG C, obtain semi-finished product, calcine 4 hours at semi-finished product being placed in Muffle furnace 200 DEG C, grinding obtains cerium acid yttrium system inorganic pigment.
Insulating moulding coating is prepared as follows:
The ethanol of S1,40 weight portions, the n-octyl alcohol of 10 weight portions, the natrium citricum of 5 weight portions, the polyethylene glycol of 4 weight portions, in the deionized water of 50 weight portions, add the nano aluminium oxide of 5 weight portions, the nano ceric oxide of 6 weight portions, the gallium-doped zinc oxide of 8 weight portions, the cerium acid yttrium system inorganic pigment of 4 weight portions, 500rpm disperses 9 minutes, then dropwise drips the silane coupler (KH570) of 10 weight portions, then use ball mill grinding 20-30 minute, make heat insulation nano composite material powdery pulp.
S2, get the polyurethane resin of 400 weight portions, add above-mentioned heat-insulating slurry, add the coating high speed dispersor of heat-insulating slurry at 800 rpm, disperse 30 minutes, then add the levelling agent of 2 weight portions, the defoamer of 1 weight portion, continue dispersion 15 minutes, be prepared into insulating moulding coating.
The present embodiment provides a kind of preparation method of organosilicon coating, comprises the steps:
The nano silicon of 5 weight portions, the nano titanium oxide of 6 weight portions joins in the deionized water of ethanol containing 20 weight portions and 30 weight portions, add the glacial acetic acid of 0.2 weight portion, drip 4 weight portion KH560 (epoxy silane coupling agent), then the polysorbas20 of 0.3 weight portion is added, the isopropyl alcohol of 1 weight portion, the defoamer of 1 weight portion, stirring at normal temperature 30min under 300-500rpm, add the organic siliconresin of 30 weight portions, stirring at normal temperature 30min under 300rpm, obtains organosilicon coating.
The present embodiment provides a kind of preparation method of rupture pressure disc, comprises the steps:
L1, algaroth preparation method: at 45 DEG C, by 20 weight portion trichloride antimonies and the mixing of 30 weight portion red fuming nitric acid (RFNA)s, slowly add 45 weight portion antimony oxides, be heated to 110 DEG C, return stirring 1 hour, cooling, filter, washing, obtains algaroth after drying.
L2, the present invention also provide a kind of preparation method of rupture pressure disc, with parts by weight, comprise the following steps: by 78 weight portion polyvinyl chloride, 8 weight portion dimethyl terephthalate (DMT)s, 12 weight portion PTTs, 5 parts by weight of polyurethane elastomers, 7 parts by weight of dimethyldimethoxysil,ne, the mixing of 6-8 parts by weight of plasticizer, stir 10-20min with the rotating speed of 800-1000 rev/min, obtain the first mixture; Described first mixture is heated to 85 DEG C, add 5-10 parts by weight of phosphoric acid triphenylmethyl methacrylate, 2 weight portion carboxyethyl phenyl phosphoric acid, 5 weight portion algaroths, nano-filled dose of 3 weight portions, 0.8 weight portion antioxidant (1010), 1 weight portion polycarboimide stabilizing agent, after stirring 30min, obtain the second mixture; Added in double screw extruder by described second mixture and carry out melt blending, extrude, cool, obtain pad pasting master batch after granulation, head temperature is 210 ~ 230 DEG C, screw speed 200 ~ 220r/min; Extrude through double screw extruder, after biaxial tension, obtain rupture pressure disc.
The preparation process of anti-flaming thermal-insulation multilayer film is as follows:
PETG diaphragm is provided;
At described PETG diaphragm surface coating acrylic acid adhesive, form acrylate glue adhensive layer;
Polyimide film is fitted on described acrylate glue adhensive layer, form polyimide layer;
At described polyimide surface successively coating thermal insulating and organosilicon coating, form heat insulating coat and organic silicon coating respectively;
Stick agent at described organic silicon coating surface coating organic silica gel, form organic silica gel adhensive layer;
Rupture pressure disc is fitted in described organosilicon adhesive surface; form explosion-proof rete; obtain anti-flaming thermal-insulation multilayer film, described anti-flaming thermal-insulation multilayer film comprises the explosion-proof rete of 1.PET diaphragm 2. acrylate glue adhensive layer 3. polyimide layer 4. heat insulating coat 5. organic silicon coating 6. organic silica gel adhensive layer 7. set gradually.
The performance of following method to anti-flaming thermal-insulation multilayer film prepared by embodiment 1-3 is adopted to measure.
The transparency test of film, adopt mist degree (Haze) and light transmittance to represent, the condition of measurement performs according to GB/T2410-2008.
Anti-flaming thermal-insulation multilayer performance measurement result prepared by table 1 embodiment of the present invention
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.